CA1316810C - Congelation fractionnee a plusieurs stades pour la surpurification de substances cristallisables - Google Patents

Congelation fractionnee a plusieurs stades pour la surpurification de substances cristallisables

Info

Publication number: CA1316810C
Authority: CA; Canada
Prior art keywords: stage; mother liquor; crystals; pure; collector
Prior art date: 1988-08-31
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.): Expired - Fee Related

Application number

CA000609630A

Other languages

English (en)

Inventor

Kenneth F. Griffiths

Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

Individual

Original Assignee

Individual

Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)

1988-08-31

Filing date

1989-08-28

Publication date

1993-04-27

1989-08-28 Application filed by Individual filed Critical Individual

1993-04-27 Application granted granted Critical

1993-04-27 Publication of CA1316810C publication Critical patent/CA1316810C/fr

2010-04-27 Anticipated expiration legal-status Critical

Status Expired - Fee Related legal-status Critical Current

Links

230000008014 freezing Effects 0.000 title claims abstract description 33
238000007710 freezing Methods 0.000 title claims abstract description 33
239000000126 substance Substances 0.000 title claims abstract description 21
239000013078 crystal Substances 0.000 claims abstract description 220
239000012452 mother liquor Substances 0.000 claims abstract description 182
238000010992 reflux Methods 0.000 claims abstract description 113
238000000034 method Methods 0.000 claims abstract description 59
238000012546 transfer Methods 0.000 claims abstract description 45
239000000463 material Substances 0.000 claims description 123
239000000047 product Substances 0.000 claims description 79
239000006227 byproduct Substances 0.000 claims description 63
230000001276 controlling effect Effects 0.000 claims description 29
238000001953 recrystallisation Methods 0.000 claims description 28
239000012535 impurity Substances 0.000 claims description 26
238000002844 melting Methods 0.000 claims description 14
230000008018 melting Effects 0.000 claims description 14
238000012545 processing Methods 0.000 claims description 6
238000005406 washing Methods 0.000 claims description 6
230000001105 regulatory effect Effects 0.000 claims description 4
239000000155 melt Substances 0.000 claims 1
WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 54
238000002425 crystallisation Methods 0.000 description 13
230000008025 crystallization Effects 0.000 description 13
239000007788 liquid Substances 0.000 description 10
239000000243 solution Substances 0.000 description 9
238000013459 approach Methods 0.000 description 7
238000011049 filling Methods 0.000 description 7
238000007670 refining Methods 0.000 description 7
230000008569 process Effects 0.000 description 6
239000004615 ingredient Substances 0.000 description 5
230000000717 retained effect Effects 0.000 description 5
238000000926 separation method Methods 0.000 description 4
UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
230000008859 change Effects 0.000 description 3
238000001816 cooling Methods 0.000 description 3
238000001640 fractional crystallisation Methods 0.000 description 3
239000000203 mixture Substances 0.000 description 3
238000000746 purification Methods 0.000 description 3
239000013014 purified material Substances 0.000 description 3
QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
238000010586 diagram Methods 0.000 description 2
238000012423 maintenance Methods 0.000 description 2
238000004519 manufacturing process Methods 0.000 description 2
238000012986 modification Methods 0.000 description 2
230000004048 modification Effects 0.000 description 2
VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical compound [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 description 2
229910001630 radium chloride Inorganic materials 0.000 description 2
238000005057 refrigeration Methods 0.000 description 2
BCNBMSZKALBQEF-UHFFFAOYSA-N 1,3-dimethylpyrrolidin-2-one Chemical compound CC1CCN(C)C1=O BCNBMSZKALBQEF-UHFFFAOYSA-N 0.000 description 1
239000005711 Benzoic acid Substances 0.000 description 1
NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
229960000583 acetic acid Drugs 0.000 description 1
239000002253 acid Substances 0.000 description 1
230000003213 activating effect Effects 0.000 description 1
238000000429 assembly Methods 0.000 description 1
230000000712 assembly Effects 0.000 description 1
WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
229910001626 barium chloride Inorganic materials 0.000 description 1
235000010233 benzoic acid Nutrition 0.000 description 1
239000004202 carbamide Substances 0.000 description 1
QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
150000001875 compounds Chemical class 0.000 description 1
239000012141 concentrate Substances 0.000 description 1
230000003247 decreasing effect Effects 0.000 description 1
230000000694 effects Effects 0.000 description 1
238000001704 evaporation Methods 0.000 description 1
230000008020 evaporation Effects 0.000 description 1
239000012530 fluid Substances 0.000 description 1
239000012362 glacial acetic acid Substances 0.000 description 1
229960000789 guanidine hydrochloride Drugs 0.000 description 1
PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 description 1
238000010438 heat treatment Methods 0.000 description 1
230000006872 improvement Effects 0.000 description 1
239000013072 incoming material Substances 0.000 description 1
150000002500 ions Chemical class 0.000 description 1
238000005259 measurement Methods 0.000 description 1
230000007246 mechanism Effects 0.000 description 1
238000002156 mixing Methods 0.000 description 1
238000012544 monitoring process Methods 0.000 description 1
238000011403 purification operation Methods 0.000 description 1
UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
239000000523 sample Substances 0.000 description 1
239000012047 saturated solution Substances 0.000 description 1
238000005204 segregation Methods 0.000 description 1
239000011734 sodium Substances 0.000 description 1
229910052708 sodium Inorganic materials 0.000 description 1
239000007787 solid Substances 0.000 description 1
YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
238000011144 upstream manufacturing Methods 0.000 description 1
238000009736 wetting Methods 0.000 description 1

Classifications

- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation

Landscapes

Chemical & Material Sciences (AREA)
Crystallography & Structural Chemistry (AREA)
Chemical Kinetics & Catalysis (AREA)
Physics & Mathematics (AREA)
Thermal Sciences (AREA)
Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Physical Water Treatments (AREA)
Steroid Compounds (AREA)
Detergent Compositions (AREA)
Fats And Perfumes (AREA)

CA000609630A 1988-08-31 1989-08-28 Congelation fractionnee a plusieurs stades pour la surpurification de substances cristallisables Expired - Fee Related CA1316810C (fr)

Applications Claiming Priority (2)

Application Number	Priority Date	Filing Date	Title
US07/238,917 US4885016A (en)	1988-08-31	1988-08-31	Multistage fractional freezing for superpurifying crystallizable substances
US238,917		1988-08-31

Publications (1)

Publication Number	Publication Date
CA1316810C true CA1316810C (fr)	1993-04-27

Family

ID=22899866

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
CA000609630A Expired - Fee Related CA1316810C (fr)	1988-08-31	1989-08-28	Congelation fractionnee a plusieurs stades pour la surpurification de substances cristallisables

Country Status (7)

Country	Link
US (1)	US4885016A (fr)
EP (1)	EP0389601B1 (fr)
JP (1)	JP2843631B2 (fr)
AT (1)	ATE112693T1 (fr)
CA (1)	CA1316810C (fr)
DE (1)	DE68918844D1 (fr)
WO (1)	WO1990001978A1 (fr)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
CA2072820A1 (fr) *	1988-07-28	1993-12-31	Kenneth F. Griffiths	Recristallisation multi-etagee pour surpurifier des substances cristallisables
US5664427A (en) *	1989-03-08	1997-09-09	Rocky Research	Rapid sorption cooling or freezing appliance
US5628205A (en) *	1989-03-08	1997-05-13	Rocky Research	Refrigerators/freezers incorporating solid-vapor sorption reactors capable of high reaction rates
US5598721A (en) *	1989-03-08	1997-02-04	Rocky Research	Heating and air conditioning systems incorporating solid-vapor sorption reactors capable of high reaction rates
US5186020A (en) *	1991-01-23	1993-02-16	Rocky Research	Portable cooler
US5240467A (en) *	1991-01-25	1993-08-31	Bicron Corporation	Multistage countercurrent recrystallization process and apparatus for performing same
US5182926A (en) *	1991-09-16	1993-02-02	Nestec S.A.	Recovery of aroma gases
US5222364A (en) *	1991-09-16	1993-06-29	Nestec S.A.	Recovery of aroma gases
US5466266A (en) *	1993-06-17	1995-11-14	Griffiths; Kenneth F.	Closed system multistage superpurification recrystallization
US8245521B2 (en) *	2007-06-20	2012-08-21	Nagarjuna Energy Private Limited	Process and apparatus for concentrating dilute solution

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
US32241A (en) *		1861-05-07		Knitting-machine
US3128188A (en) *	1960-09-02	1964-04-07	Union Carbide Corp	Beer lagering process
NL132874C (fr) *	1962-07-05
AT279547B (de)	1967-04-14	1970-03-10	Buchs Metallwerk Ag	Verfahren und Vorrichtung zur Trennung oder Reinigung schmelzflüssiger, flüssiger oder gelöster Stoffe durch fraktioniertes Kristallisieren
US3992900A (en) *	1973-03-27	1976-11-23	Avco Corporation	Plural stage freeze crystallization with wash-water/concentrate interface control
US4143524A (en) *	1974-12-06	1979-03-13	Douwe Egberts Koninklijke Tabaksfabriek-Koffiebranderijen-Theehandel B.V.	Process and apparatus for separating crystallizable materials from a multi-component system
ZA80554B (en) *	1979-02-22	1981-02-25	Douwe Egberts Tabaksfab	Counter current crystallization process
US4430104A (en) *	1980-10-30	1984-02-07	Grasso's Koniklijke Machine Fabrieken, N.V.	Multi-stage countercurrent concentrating system and method and separator
US4406679A (en) *	1981-09-21	1983-09-27	Concentration Specialists, Inc.	Apparatus for and method of preparing crystals for washing
NL8200075A (nl) *	1982-01-11	1983-08-01	Tno	Werkwijze voor het continu gedeeltelijk kristaliseren en het scheiden van een vloeibaar mengsel en een inrichting voor het uitvoeren van deze werkwijze.
US4557741A (en) *	1984-02-13	1985-12-10	Grasso's Koniklyke Machine Fabriekon N.V.	Gradient column freeze concentration system

1988
- 1988-08-31 US US07/238,917 patent/US4885016A/en not_active Expired - Fee Related
1989
- 1989-08-24 AT AT89910394T patent/ATE112693T1/de active
- 1989-08-24 WO PCT/US1989/003669 patent/WO1990001978A1/fr not_active Ceased
- 1989-08-24 JP JP1509703A patent/JP2843631B2/ja not_active Expired - Lifetime
- 1989-08-24 DE DE68918844T patent/DE68918844D1/de not_active Expired - Lifetime
- 1989-08-24 EP EP89910394A patent/EP0389601B1/fr not_active Expired - Lifetime
- 1989-08-28 CA CA000609630A patent/CA1316810C/fr not_active Expired - Fee Related

Also Published As

Publication number	Publication date
ATE112693T1 (de)	1994-10-15
JP2843631B2 (ja)	1999-01-06
WO1990001978A1 (fr)	1990-03-08
EP0389601A4 (en)	1991-09-25
DE68918844D1 (de)	1994-11-17
US4885016A (en)	1989-12-05
EP0389601B1 (fr)	1994-10-12
JPH03501824A (ja)	1991-04-25
EP0389601A1 (fr)	1990-10-03

Legal Events

Date	Code	Title	Description
2000-04-27	MKLA	Lapsed
2023-05-26	MKLA	Lapsed	Effective date: 20000427

Publication	Publication Date	Title
USRE32241E (en)	1986-09-09	Fractional crystallization process
JP3909364B2 (ja)	2007-04-25	ガリウムの精製方法および装置
US4588414A (en)	1986-05-13	Countercurrent, cooling crystallization and purification method for multi-component molten mixture
US4885016A (en)	1989-12-05	Multistage fractional freezing for superpurifying crystallizable substances
US4666456A (en)	1987-05-19	Process for the continuous partial crystallization and the separation of a liquid mixture
US5127921A (en)	1992-07-07	Multistage recrystallization for superpurifying crystallizable substances
CN107750181A (zh)	2018-03-02	半连续结晶方法和装置
US3375082A (en)	1968-03-26	Process for the continuous separation of crystallizable substances
US5814231A (en)	1998-09-29	Separation of liquid eutectic mixtures by crystallization on cold surfaces and apparatus for this purpose
US4406679A (en)	1983-09-27	Apparatus for and method of preparing crystals for washing
Ulrich et al.	1996	Solid layer melt crystallization
US4453959A (en)	1984-06-12	Crystal washing and purification method
JPS63185402A (ja)	1988-08-01	液状混合物から純粋な物質を結晶化によつて回収する方法および装置
JPH09103604A (ja)	1997-04-22	晶出により液体混合物から物質を分離する方法
JPS6025504A (ja)	1985-02-08	結晶精製装置
US5466266A (en)	1995-11-14	Closed system multistage superpurification recrystallization
EP0576718B1 (fr)	1996-09-25	Cristallisation en étapes multiples pour la purification de produits cristallisables
US5090965A (en)	1992-02-25	Process for the separation of substances by cooling crystallization
US4670611A (en)	1987-06-02	Method and installation for the crystallization of mannitol
US3541804A (en)	1970-11-24	Fractional crystallization with an immiscible refrigerant
JP2001505485A (ja)	2001-04-24	懸濁結晶化法
IE922200A1 (en)	1994-01-12	Multistage recrystallization for superpurifying¹crystallizable substances
Ulrich et al.	1995	Melt layer crystallization
US6454853B1 (en)	2002-09-24	Process for the purification of organic products by fractionated crystallization at a variable circulation rate
JPH0631105A (ja)	1994-02-08	結晶化可能な物質を超精製する多段階再結晶化